The isometric, pyrochlore structure type, A2B2O7, exhibits a wide variety of properties that find application in a large number of different technologies, from electrolytes in solid oxide fuel cells to actinide-bearing compositions that can be used as nuclear waste forms or inert matrix nuclear fuels. Swift xenon ions (1.43 GeV) have been used to systematically modify different compositions in the Gd2Zr2-xTixO7 binary at the nanoscale by radiation-induced phase transitions that include the crystalline-to-amorphous and order-disorder structural transformations. Synchrotron x-ray diffraction, Raman spectroscopy, and transmission electron microscopy provide a complete and consistent description of structural changes induced by the swift heavy ions and demonstrate that the response of pyrochlore depends strongly on chemical composition. The high and dense electronic energy deposition primarily results in amorphization of Ti-rich pyrochlore; whereas the formation of the fully disordered, defect-fluorite structure is the dominant process for Zr-rich pyrochlore.

Using a spherical aberration (Cs)-corrected scanning transmission electron microscopy (STEM) and electron energy-loss spectroscopy (EELS), we investigated a 6° low-angle [001] tilt grain boundary in SrTiO3. The enhanced spatial resolution of the aberration corrector leads to the observation of a number of structural variations in the edge dislocations along the grain boundary that neither resemble the standard edge dislocations nor partial dislocations for SrTiO3. Although there appear to be many variants in the structure that can be interpreted as compositional effects, three main classes of core structure are found to be prominent. From EELS analysis, these classifications seem to be related to Sr deficiencies, with the final variety of the cores being consistent with an embedded TiOx rocksalt-like structure.

Uniform monodisperse nanospheres of tetra-kis(4-methoxylphenyl) porphynatemanganese (III) chloride [MnIII(TMOPP)Cl] of about 200 nm have been synthesized through a facile surfactant-assisted reprecipitation method at room temperature. Scanning electron microscopy, transmission electron microscope, infrared spectrum, ultraviolet–visible spectrum, and elemental analysis were adopted to characterize the as-prepared metalloporphyrin nanostructures. The influence factors in the reaction to the sizes and morphologies of porphyrin nanoparticles were discussed. The sizes of porphyrin nanoparticles were affected mainly by the porphyrin concentration and only monodisperse nanoshperes with high uniformity in sizes and shapes can self-assemble to form order two-dimensional superstructures.

Scanning electron microscopy and transmission electron microscopy images and selected area electron diffraction pattern showed that the one-dimensional GaN nanorods with [0001]-oriented single-crystalline wurzite structures were formed on Si (111) substrates by using hydride vapor-phase epitaxy without a catalyst. Although some stacking faults and inversion domain boundaries existed in the GaN nanorods, few other defects such as threading dislocations were observed. The formation of the facet plane in the N-polar region of the GaN nanorod containing an inversion domain boundary originated from the slow growth rate, followed by the lateral adatom diffusion from the Ga-polar region to reduce the length difference.

This study proposes a method developed to simultaneously solve contact hardness and reduced modulus by loading and unloading coefficients together with the inclined angle of an indenter. The ratios of the applied load to the squared slopes of load–depth curves during loading and unloading processes were used to determine loading and unloading coefficients. The values of the contact area estimated by the present method were found to be precise for a variety of materials. Compared to the reduced modulus, errors due to underestimated contact area were found more significant in the evaluation of contact hardness.

(Ti1–xSix)Ny (0 ≤ x ≤ 0.20; 0.99 ≤ y(x) ≤ 1.13) thin films deposited by arc evaporation have been investigated by analytical transmission electron microscopy, x-ray diffraction, x-ray photoelectron spectroscopy, and nanoindentation. Films with x ≤ 0.09 are single-phase cubic (Ti,Si)N solid solutions with a dense columnar microstructure. Films with x > 0.09 have a featherlike microstructure consisting of cubic TiN:Si nanocrystallite bundles separated by metastable SiNz with coherent-to-semicoherent interfaces and a dislocation density of as much as 1014 cm−2 is present. The films exhibit retained composition and hardness between 31 and 42 GPa in annealing experiments to 1000 °C due to segregation of SiNz to the grain boundaries. During annealing at 1100–1200 °C, this tissue phase thickens and transforms to amorphous SiNz. At the same time, Si and N diffuse out of the films via the grain boundaries and TiN recrystallize.

Cr3+/Ni2+ co-doped optically transparent magnesium aluminosilicate glass-ceramics containing MgAl2O4 nanocrystals have been prepared by heat-treatment. Greatly enhanced broadband near-infrared emission centered at 1216 nm in Cr3+/Ni2+ co-doped glass ceramics is observed when compared with the Ni2+ single-doped glass ceramics under 532 nm excitation. The observed enhancement of infrared emission is attributed to the energy transfer from Cr3+ to Ni2+ ions in the nanocrystalline phase, which leads to the emission due to 3T2(3F) → 3A2(3F) transition of octahedral Ni2+ ions.

The role of high current stressing during growth of the P-rich phase at the electroless Ni/Sn interface was examined by transmission electron microscopy. Prior to current stressing, two layers of Ni12P5, columnar Ni12P5 and noncolumnar Ni12P5, were formed after soldering. Upon electric stressing, the two layers of P-rich phase showed opposite growth patterns at the two opposing electrode interfaces. At the cathode, columnar growth of the P-rich phase was greatly enhanced while growth of the noncolumnar layer was inhibited. By contrast, the opposite was found at the anode where the current stressing promoted the noncolumnar growth but suppressed the growth of the columnar layer. Such a strong polarity effect resulted from directional electromigration of the key reaction species, nickel, to and from the interfacial reaction fronts. As a result of the difference in reaction mechanism, overall growth of the P-rich phase was much faster at the cathode during current stressing.

The clean and ordered surfaces of CdZnTe (111)B grown by the Bridgman method were obtained by Ar ion bombardment and thermal annealing in situ in an ultrahigh vacuum. The surface atomic structures of CdZnTe (111)B after annealing at different temperature were observed by low-energy electron diffraction (LEED). The valence band and work function of CdZnTe (111)B surfaces were determined by synchrotron radiation photoemission spectroscopy. The order of CdZnTe (111)B after annealing at 350 °C will worsen, and the (111)B-(2 × 2) local reconstruction will be formed. The work function of CdZnTe (111)B after annealing at 350 °C is 0.8 eV higher than that of CdZnTe (111)B-(1 × 1), and the local reconstruction may be induced by Te adatoms on top of the ideal truncation.

NaGd(MoO4)2:Ln3+ (Ln = Eu, Tb) submicrometer phosphors have been synthesized by a composite method including the solid state reaction process at room temperature and the hydrothermal process. It is revealed that temperature and humidity have an influence on the reaction rate and that higher temperature and humidity can speed up the reaction process. Crystalline water is necessary for the solid phase reaction at room temperature. The x-ray diffraction (XRD) patterns indicate that NaGd(MoO4)2:Ln3+ (Ln = Eu, Tb) submicrometer phosphors crystallize well with the scheelite structure. Both scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images illustrate that the average grain size of NaGd(MoO4)2:Ln3+ is about 225 nm without conglomeration. The luminescent lifetime and quantum efficiency for NaGd(MoO4)2:Eu3+ are determined.

In situ observation of tin whisker growth in NdSn3 compound was carried out by using an optical microscope (OM) and scanning electron microscopy (SEM). The growth rate of Sn-whisker from NdSn3 is shown to be rapid (approximately 8-15Å/s) during exposure to room ambience, and it is accompanied by formation of a new compound, Nd(OH)3, as was confirmed by x-ray diffraction. This reaction between the Sn-RE compound and trace water in room ambience has significant influence on whisker growth. There is an electron irradiation effect on whisker growth; that is, whiskers stopped growing after being observed in SEM. Therefore, it is suggested that OM be used rather than SEM to observe the continuous whisker growth. In discussion, the driving force per Sn atom for whisker growth is estimated as 1 × 1014 N in accordance with the whisker growth rate, and its apparent force originates from a chemical potential gradient between the released Sn atoms and the whisker.

Nanoindentation was undertaken near grain boundaries to increase understanding of their individual contributions to the material’s macroscopic mechanical properties. Prior work with nanoindentation in body-centered cubic (bcc) materials has shown that some grain boundaries produce a “pop-in” event, an excursion in the load–displacement curve. In the current work, grain boundary associated pop-in events were observed in a Fe–0.01 wt% C polycrystal (bcc), and this is characteristic of high resistance to intergranular slip transfer. Grain boundaries with greater misalignment of slip systems tended to exhibit greater resistance to slip transfer. Grain boundary associated pop-ins were not observed in pure copper (face-centered cubic) or interstitial free steel ~0.002 wt% C (bcc). Additionally, it was found that cold work of the Fe–0.01 wt% C polycrystal immediately prior to indentation completely suppressed grain boundary associated pop-in events. It is concluded that the grain boundary associated pop-in events are directly linked to interstitials pinning dislocations on or near the boundary. This links well with macroscopic Hall–Petch effect observations.

The process of ultrathin Al-induced crystallization of amorphous Si (a-Si) has been investigated by using high-resolution transmission electron microscopy and Auger electron spectroscopic depth profiling. Ultrathin Al overlayers, with thicknesses of 2.0 and 4.5 nm, have been shown to be capable of inducing full crystallization of an a-Si bottom layer as thick as 40 nm at temperatures as low as 320 °C. After full crystallization of a-Si, the Al of the original 2.0-nm Al overlayer completely moved through the Si layer, leaving a high-purity, large-grained crystalline Si layer above it. Such movement of Al also occurs for the originally 4.5-nm Al overlayer, but in this case the crystallized Si layer is relatively fine-grained and contains ∼5.0 at.% of residual Al nanocrystals distributed throughout the layer. The observations have been interpreted on the basis of sites available for nucleation of crystalline Si in the microstructure of the Al/Si layer system upon annealing.

The effect of Li3N additive on the Li-Mg-N-H system was examined with respect to the reversible dehydrogenation performance. Screening study with varying Li3N additions (5, 10, 20, and 30 mol%) demonstrates that all are effective for improving the hydrogen desorption capacity. Optimally, incorporation of 10 mol% Li3N improves the practical capacity from 3.9 wt% to approximately 4.7 wt% hydrogen at 200 °C, which drives the dehydrogenation reaction toward completion. Moreover, the capacity enhancement persists well over 10 de-/rehydrogenation cycles. Systematic x-ray diffraction examinations indicate that Li3N additive transforms into LiNH2 and LiH phases and remains during hydrogen cycling. Combined structure/property investigations suggest that the LiNH2 “seeding” should be responsible for the capacity enhancement, which reduces the kinetic barrier associated with the nucleation of intermediate LiNH2. In addition, the concurrent incorporation of LiH is effective for mitigating the ammonia release.

A first-principles method was used to investigate the structural and energetic properties for A2Ti2O7 (A = Lu, Er, Y, Gd, Sm, Nd, La), including the formation energies of the cation antisite-pair, the anion Frenkel pair that defines anion-disorder, and the coupled cation antisite-pair/anion-Frenkel. It is proposed that the 〈A–O48f〉 interaction may have more significant influence on the radiation resistance behavior of titanate pyrochlores, although the 〈Ti–O48f〉 interactions are relatively stronger than the 〈A–O48f〉 interactions. It was found that the defect formation energies are not simple functions of the A-site cation radii. The formation energy of the cation antisite-pair increases continuously as the A-site cation varies from Lu to Gd, and then decreases continuously with the variation of the A-site cation from Gd to La, in excellent agreement with the radiation-resistance trend of the titanate pyrochlores. The band gaps in these pyrochlores were also measured, and the band gap widths changed continuously with cation radius.

Ferroelectric K0.5Na0.5NbO3 (KNN) thin films were prepared by a chemical solution deposition approach with polyvinylpyrrolidone (PVP) of different molecular weights introduced in the precursor solutions. The volatilization of the alkali ions and the effects of the molecular weight of PVP were examined with x-ray diffraction (XRD), thermal analysis, mass spectrometry, and x-ray photoelectron spectroscopy (XPS). The results clearly showed that the volatilization of the alkali ions mainly happened at moderate temperatures before the crystallization of the KNN perovskite phase. Loss of Na was more significant than K ions during the heating process of KNN. The introduction of PVP with the appropriate molecular weight could effectively promote the crystallization of the KNN perovskite phase at reduced temperature and substantially suppress the loss of the alkali ions before crystallization. Therefore, a high dielectric constant, piezoelectric coefficient, and well saturated ferroelectric hysteresis loops were obtained in the KNN films in which PVP of the right molecular weight were introduced.

Individual triangular/hexagonal nanoplates, chain-like nanoplate assemblies, and nanobelts in the case of silver were selectively synthesized using N,N-dimethylformamide (DMF) in the presence of poly (vinyl pyrrolidone) (PVP). The molar ratio of AgNO3/PVP, concentration of AgNO3, temperature, and process time were crucial factors in determining the morphologies of the final products. Based on the experimental results, it was concluded that the products were favorable to form individual nanoplates because of the strong interaction between PVP and Ag+, and the outline of the nanoplates was controlled by the ratio of AgNO3 and PVP. The formation of novel chain-like nanoplate assemblies could be explained by the secondary growth of the nanocrystals. If the reaction continuously lasted for another 7 h, the chain-like assemblies could transform into nanobelts with width of 40∼100 nm and the length of several micrometers.

Nanoscale surface texturing of silicon was accomplished by oblique Ar+ ion beam irradiation. Atomic force microscope (AFM) imaging showed that nanotexturing produced an anisotropic morphology consisting of ordered nanometer-sized ripples. Surface force microscope (SFM) measurements showed that the nanotextured surface exhibited scale-dependent nanomechanical behavior during indentation loading/unloading and anisotropic sliding friction, significantly different from those of the original (untextured) surface. AFM and SFM results showed a strong dependence of the nanoindentation response and friction coefficient on the tip radius and sliding direction relative to the ripple orientation. The observed experimental trends are interpreted in terms of the applied normal load, real contact area, interfacial adhesion force, tip-ripple interaction scale, and ripple orientation.

Bulk metallic glasses (BMGs) with high thermal stability and good corrosion resistance were synthesized in the (Cu0.6Hf0.25Ti0.15)100−x−yNiyNbx system by copper mold casting. The addition of Ni element causes an extension of a supercooled liquid region (ΔTx = Tx – Tg) from 60 K for Cu60Hf25Ti15 to 70 K for (Cu0.6Hf0.25Ti0.15)95Ni5. The simultaneous addition of Ni and Nb to the alloy is effective in improving synergistically the corrosion resistance in 1 N HCl, 3 mass% NaCl, and 1 N H2SO4 + 0.01 N NaCl solutions. The highly protective Hf-, Ti-, and Nb-enriched surface film is formed by the rapid initial preferential dissolution of Cu and Ni, which is responsible for the high corrosion resistance of the alloys in the solutions examined.

Hydroxyapatite (HAp) and brushite (DCPD) are two important compounds of the calcium apatite family with excellent bioactivity and osteoconductive properties in vivo. This work aimed to investigate the stability of HAp nanorods synthesized by the hydrothermal method in acetic acid aqueous solution. The results illuminated that HAp nanorods were converted into hollow nanospheres, and it was found that the concentration and amount of the acetic acid and the reaction time significantly affected the degree of the morphological evolution. Transmission electron microscope, high-resolution transmission electron microscope, and x-ray diffraction were performed for characterizing the samples.